#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:38:46 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179855 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/51/7015191.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7015191
loop_
_publ_author_name
'Santana, M. Dolores'
'García-Bueno, Rocío'
'García, Gabriel'
'Sánchez, Gregorio'
'García, Joaquín'
'Pérez, José'
'García, Luis'
'Serrano, J. Luis'
_publ_section_title
;
 Synthesis and luminescence properties of cyclopalladated complexes
 with S^N and O^N donor ligands.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              3537
_journal_page_last               3546
_journal_paper_doi               10.1039/c0dt01337d
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C35 H27 Cl3 N6 Pd2 S2'
_chemical_formula_weight         914.90
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 106.0290(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8956(4)
_cell_length_b                   28.7252(12)
_cell_length_c                   12.3772(5)
_cell_measurement_temperature    100(2)
_cell_volume                     3381.5(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.941
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0282
_diffrn_reflns_av_sigmaI/netI    0.0231
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            38970
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    1.461
_exptl_absorpt_correction_T_max  0.9046
_exptl_absorpt_correction_T_min  0.7998
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   SADABS
_exptl_crystal_density_diffrn    1.797
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.763
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.179
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     437
_refine_ls_number_reflns         7845
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.179
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0432
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0347P)²+10.6297P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.0988
_reflns_number_gt                7459
_reflns_number_total             7845
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt01337d.txt
_cod_data_source_block           complexII3
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7015191
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Pd1 Pd 0.99066(3) 0.158388(9) 0.71895(2) 0.01761(8) Uani 1 1 d . . .
Pd2 Pd 1.14242(3) 0.087499(10) 0.87630(2) 0.02054(8) Uani 1 1 d . . .
S2 S 1.33274(10) 0.09680(4) 0.80486(8) 0.0284(2) Uani 1 1 d . . .
Cl1 Cl 1.46312(12) -0.01502(4) 0.80334(10) 0.0411(3) Uani 1 1 d . . .
Cl2 Cl 1.70335(12) -0.04728(4) 0.73582(11) 0.0414(3) Uani 1 1 d . . .
Cl3 Cl 1.44614(13) -0.10193(4) 0.68282(11) 0.0456(3) Uani 1 1 d . . .
S1 S 0.82998(10) 0.10351(3) 0.62879(8) 0.0254(2) Uani 1 1 d . . .
N1 N 1.1199(3) 0.21118(10) 0.8022(3) 0.0195(6) Uani 1 1 d . . .
N2 N 1.1316(3) 0.13649(10) 0.6250(3) 0.0226(6) Uani 1 1 d . . .
N4 N 0.9837(3) 0.08285(11) 0.9555(3) 0.0232(6) Uani 1 1 d . . .
N6 N 0.8866(3) 0.01359(11) 0.5929(3) 0.0239(6) Uani 1 1 d . . .
N5 N 1.0363(3) 0.04255(11) 0.7437(3) 0.0245(7) Uani 1 1 d . . .
C16 C 1.1168(4) 0.14415(14) 0.5155(3) 0.0267(8) Uani 1 1 d . . .
H16 H 1.0383 0.1589 0.4655 0.032 Uiso 1 1 calc R . .
C12 C 0.9322(4) 0.21788(12) 0.8850(3) 0.0189(7) Uani 1 1 d . . .
C13 C 1.0678(4) 0.23293(12) 0.8802(3) 0.0187(7) Uani 1 1 d . . .
C27 C 1.3502(4) 0.15596(14) 1.0330(4) 0.0293(8) Uani 1 1 d . . .
H27 H 1.4163 0.1518 0.9909 0.035 Uiso 1 1 calc R . .
C8 C 0.7345(4) 0.22507(14) 0.9623(3) 0.0260(8) Uani 1 1 d . . .
H8 H 0.6885 0.2392 1.0119 0.031 Uiso 1 1 calc R . .
C21 C 0.9038(4) 0.11941(15) 1.1034(3) 0.0288(8) Uani 1 1 d . . .
C11 C 0.8667(4) 0.18181(12) 0.8109(3) 0.0183(7) Uani 1 1 d . . .
C28 C 1.2257(4) 0.13098(13) 1.0031(3) 0.0227(7) Uani 1 1 d . . .
C31 C 0.9254(4) 0.05199(13) 0.6574(3) 0.0213(7) Uani 1 1 d . . .
C1 C 1.2471(4) 0.22356(13) 0.7956(3) 0.0241(8) Uani 1 1 d . . .
H1 H 1.2846 0.2086 0.7418 0.029 Uiso 1 1 calc R . .
C7 C 0.8702(4) 0.23935(13) 0.9623(3) 0.0222(7) Uani 1 1 d . . .
C30 C 1.0041(4) 0.11310(13) 1.0440(3) 0.0227(7) Uani 1 1 d . . .
N3 N 1.3186(3) 0.10853(11) 0.5840(3) 0.0242(7) Uani 1 1 d . . .
C14 C 1.2556(4) 0.11441(13) 0.6681(3) 0.0210(7) Uani 1 1 d . . .
C29 C 1.1328(4) 0.13841(13) 1.0706(3) 0.0221(7) Uani 1 1 d . . .
C6 C 0.9486(4) 0.27467(14) 1.0357(3) 0.0283(8) Uani 1 1 d . . .
H6 H 0.9082 0.2890 1.0886 0.034 Uiso 1 1 calc R . .
C4 C 1.1415(4) 0.26782(13) 0.9519(3) 0.0252(8) Uani 1 1 d . . .
C10 C 0.7344(4) 0.16871(14) 0.8164(3) 0.0245(8) Uani 1 1 d . . .
H10 H 0.6866 0.1444 0.7691 0.029 Uiso 1 1 calc R . .
C32 C 0.9766(4) -0.02233(14) 0.6414(4) 0.0309(9) Uani 1 1 d . . .
H32 H 0.9746 -0.0536 0.6157 0.037 Uiso 1 1 calc R . .
C24 C 1.1609(4) 0.16994(14) 1.1611(3) 0.0272(8) Uani 1 1 d . . .
C20 C 0.7781(5) 0.09396(16) 1.0685(4) 0.0347(10) Uani 1 1 d . . .
H20 H 0.7066 0.0978 1.1056 0.042 Uiso 1 1 calc R . .
C5 C 1.0775(4) 0.28807(14) 1.0317(3) 0.0288(8) Uani 1 1 d . . .
H5 H 1.1267 0.3112 1.0822 0.035 Uiso 1 1 calc R . .
C22 C 0.9353(5) 0.15226(16) 1.1949(4) 0.0340(9) Uani 1 1 d . . .
H22 H 0.8694 0.1573 1.2368 0.041 Uiso 1 1 calc R . .
C26 C 1.3815(5) 0.18720(15) 1.1237(4) 0.0336(9) Uani 1 1 d . . .
H26 H 1.4680 0.2037 1.1416 0.040 Uiso 1 1 calc R . .
C9 C 0.6690(4) 0.19063(15) 0.8903(3) 0.0279(8) Uani 1 1 d . . .
H9 H 0.5769 0.1813 0.8902 0.034 Uiso 1 1 calc R . .
C3 C 1.2758(4) 0.27979(14) 0.9427(4) 0.0310(9) Uani 1 1 d . . .
H3 H 1.3299 0.3030 0.9901 0.037 Uiso 1 1 calc R . .
C17 C 1.4550(4) 0.08821(15) 0.5940(4) 0.0321(9) Uani 1 1 d . . .
H17A H 1.4740 0.0883 0.5204 0.048 Uiso 1 1 calc R . .
H17B H 1.4562 0.0561 0.6210 0.048 Uiso 1 1 calc R . .
H17C H 1.5273 0.1064 0.6474 0.048 Uiso 1 1 calc R . .
C25 C 1.2892(5) 0.19431(15) 1.1869(4) 0.0343(9) Uani 1 1 d . . .
H25 H 1.3118 0.2156 1.2480 0.041 Uiso 1 1 calc R . .
C2 C 1.3274(4) 0.25766(14) 0.8649(4) 0.0299(9) Uani 1 1 d . . .
H2 H 1.4179 0.2655 0.8579 0.036 Uiso 1 1 calc R . .
C15 C 1.2304(4) 0.12766(14) 0.4869(3) 0.0283(8) Uani 1 1 d . . .
H15 H 1.2466 0.1289 0.4148 0.034 Uiso 1 1 calc R . .
C18 C 0.8646(4) 0.05866(15) 0.9261(3) 0.0312(9) Uani 1 1 d . . .
H18 H 0.8504 0.0372 0.8656 0.037 Uiso 1 1 calc R . .
C33 C 1.0683(4) -0.00352(14) 0.7334(4) 0.0294(8) Uani 1 1 d . . .
H33 H 1.1436 -0.0198 0.7834 0.035 Uiso 1 1 calc R . .
C23 C 1.0584(5) 0.17605(16) 1.2214(3) 0.0337(9) Uani 1 1 d . . .
H23 H 1.0770 0.1975 1.2822 0.040 Uiso 1 1 calc R . .
C34 C 0.7680(4) 0.01010(15) 0.4930(4) 0.0314(9) Uani 1 1 d . . .
H34A H 0.7635 -0.0215 0.4623 0.047 Uiso 1 1 calc R . .
H34B H 0.7798 0.0325 0.4366 0.047 Uiso 1 1 calc R . .
H34C H 0.6808 0.0169 0.5129 0.047 Uiso 1 1 calc R . .
C19 C 0.7598(5) 0.06362(16) 0.9808(4) 0.0357(10) Uani 1 1 d . . .
H19 H 0.6757 0.0459 0.9570 0.043 Uiso 1 1 calc R . .
C35 C 1.5576(5) -0.06492(16) 0.7817(4) 0.0329(9) Uani 1 1 d . . .
H35 H 1.591(5) -0.0804(18) 0.853(4) 0.038(13) Uiso 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Pd Pd -0.9988 1.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C11 Pd1 N1 82.08(13) . . ?
C11 Pd1 N2 176.66(13) . . ?
N1 Pd1 N2 94.58(12) . . ?
C11 Pd1 S1 93.22(10) . . ?
N1 Pd1 S1 174.78(9) . . ?
N2 Pd1 S1 90.11(9) . . ?
C11 Pd1 Pd2 97.90(10) . . ?
N1 Pd1 Pd2 92.62(8) . . ?
N2 Pd1 Pd2 82.27(8) . . ?
S1 Pd1 Pd2 90.28(3) . . ?
C28 Pd2 N4 82.55(14) . . ?
C28 Pd2 N5 174.94(14) . . ?
N4 Pd2 N5 92.80(13) . . ?
C28 Pd2 S2 91.47(12) . . ?
N4 Pd2 S2 173.92(9) . . ?
N5 Pd2 S2 93.21(9) . . ?
C28 Pd2 Pd1 96.45(10) . . ?
N4 Pd2 Pd1 92.47(9) . . ?
N5 Pd2 Pd1 81.69(9) . . ?
S2 Pd2 Pd1 89.29(3) . . ?
C14 S2 Pd2 102.86(13) . . ?
C31 S1 Pd1 102.78(13) . . ?
C1 N1 C13 117.9(3) . . ?
C1 N1 Pd1 129.1(3) . . ?
C13 N1 Pd1 112.7(2) . . ?
C16 N2 C14 108.0(3) . . ?
C16 N2 Pd1 126.5(3) . . ?
C14 N2 Pd1 125.4(3) . . ?
C18 N4 C30 118.3(3) . . ?
C18 N4 Pd2 129.4(3) . . ?
C30 N4 Pd2 112.0(2) . . ?
C31 N6 C32 107.9(3) . . ?
C31 N6 C34 126.0(3) . . ?
C32 N6 C34 126.0(3) . . ?
C31 N5 C33 106.3(3) . . ?
C31 N5 Pd2 128.2(3) . . ?
C33 N5 Pd2 125.4(3) . . ?
N2 C16 C15 109.9(4) . . ?
C7 C12 C11 123.5(3) . . ?
C7 C12 C13 119.0(3) . . ?
C11 C12 C13 117.6(3) . . ?
N1 C13 C4 122.9(3) . . ?
N1 C13 C12 115.7(3) . . ?
C4 C13 C12 121.5(3) . . ?
C28 C27 C26 121.9(4) . . ?
C9 C8 C7 119.4(3) . . ?
C30 C21 C20 117.9(4) . . ?
C30 C21 C22 117.8(4) . . ?
C20 C21 C22 124.3(4) . . ?
C10 C11 C12 116.0(3) . . ?
C10 C11 Pd1 132.2(3) . . ?
C12 C11 Pd1 111.7(2) . . ?
C27 C28 C29 116.0(4) . . ?
C27 C28 Pd2 132.6(3) . . ?
C29 C28 Pd2 111.3(3) . . ?
N5 C31 N6 110.1(3) . . ?
N5 C31 S1 128.1(3) . . ?
N6 C31 S1 121.6(3) . . ?
N1 C1 C2 122.5(4) . . ?
C8 C7 C12 117.8(3) . . ?
C8 C7 C6 123.7(3) . . ?
C12 C7 C6 118.5(3) . . ?
N4 C30 C21 122.2(4) . . ?
N4 C30 C29 115.7(3) . . ?
C21 C30 C29 122.1(4) . . ?
C14 N3 C15 107.5(3) . . ?
C14 N3 C17 126.7(3) . . ?
C15 N3 C17 125.7(3) . . ?
N2 C14 N3 108.3(3) . . ?
N2 C14 S2 129.0(3) . . ?
N3 C14 S2 122.7(3) . . ?
C24 C29 C28 123.2(4) . . ?
C24 C29 C30 118.7(4) . . ?
C28 C29 C30 118.1(3) . . ?
C5 C6 C7 122.0(4) . . ?
C13 C4 C3 117.5(4) . . ?
C13 C4 C5 118.3(3) . . ?
C3 C4 C5 124.2(4) . . ?
C11 C10 C9 121.5(4) . . ?
C33 C32 N6 105.5(3) . . ?
C25 C24 C29 118.0(4) . . ?
C25 C24 C23 123.1(4) . . ?
C29 C24 C23 118.9(4) . . ?
C19 C20 C21 119.2(4) . . ?
C6 C5 C4 120.8(4) . . ?
C23 C22 C21 120.4(4) . . ?
C25 C26 C27 121.1(4) . . ?
C8 C9 C10 121.8(3) . . ?
C2 C3 C4 119.2(4) . . ?
C26 C25 C24 119.8(4) . . ?
C3 C2 C1 120.0(4) . . ?
C16 C15 N3 106.3(3) . . ?
N4 C18 C19 122.4(4) . . ?
C32 C33 N5 110.1(4) . . ?
C22 C23 C24 122.2(4) . . ?
C20 C19 C18 119.9(4) . . ?
Cl3 C35 Cl2 111.1(3) . . ?
Cl3 C35 Cl1 109.7(2) . . ?
Cl2 C35 Cl1 109.2(2) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Pd1 C11 2.006(3) . ?
Pd1 N1 2.066(3) . ?
Pd1 N2 2.141(3) . ?
Pd1 S1 2.2976(10) . ?
Pd1 Pd2 2.9291(4) . ?
Pd2 C28 1.997(4) . ?
Pd2 N4 2.073(3) . ?
Pd2 N5 2.124(3) . ?
Pd2 S2 2.3064(11) . ?
S2 C14 1.729(4) . ?
Cl1 C35 1.772(5) . ?
Cl2 C35 1.764(5) . ?
Cl3 C35 1.761(5) . ?
S1 C31 1.738(4) . ?
N1 C1 1.332(5) . ?
N1 C13 1.366(5) . ?
N2 C16 1.341(5) . ?
N2 C14 1.353(5) . ?
N4 C18 1.330(5) . ?
N4 C30 1.369(5) . ?
N6 C31 1.353(5) . ?
N6 C32 1.387(5) . ?
N6 C34 1.454(5) . ?
N5 C31 1.332(5) . ?
N5 C33 1.375(5) . ?
C16 C15 1.354(6) . ?
C12 C7 1.413(5) . ?
C12 C11 1.416(5) . ?
C12 C13 1.427(5) . ?
C13 C4 1.402(5) . ?
C27 C28 1.385(5) . ?
C27 C26 1.403(6) . ?
C8 C9 1.369(6) . ?
C8 C7 1.405(5) . ?
C21 C30 1.400(6) . ?
C21 C20 1.404(6) . ?
C21 C22 1.440(6) . ?
C11 C10 1.381(5) . ?
C28 C29 1.418(5) . ?
C1 C2 1.396(6) . ?
C7 C6 1.438(6) . ?
C30 C29 1.424(5) . ?
N3 C14 1.363(5) . ?
N3 C15 1.388(5) . ?
N3 C17 1.444(5) . ?
C29 C24 1.407(5) . ?
C6 C5 1.347(6) . ?
C4 C3 1.407(6) . ?
C4 C5 1.435(5) . ?
C10 C9 1.407(5) . ?
C32 C33 1.356(6) . ?
C24 C25 1.407(6) . ?
C24 C23 1.427(6) . ?
C20 C19 1.365(7) . ?
C22 C23 1.355(6) . ?
C26 C25 1.373(7) . ?
C3 C2 1.365(6) . ?
C18 C19 1.393(6) . ?
